반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][CH2:10][C:11]([OH:13])=O>O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]2[C:3]=1[CH2:9][CH2:10][C:11]2=[O:13]참가 물질
3
실험 절차
3-(2,4-dichlorophenyl)propanoic acid (0.44 g, 2 mmol) in polyphosphoric acid (7 g) was heated to 100° C. under argon. After 90 min the mixture was cooled and treated with water (20 ml) and extracted with hexane (40 ml). The hexane layer was dried (MgSO4), and evaporated to dryness. The residue was purified by column chromatography on silica gel eluting with 0-30% dichloromethane in hexane to give the title product as a yellow solid, (0.018 g, 4.5%), δH (CDCl3) 2.8 (2H, m), 3.1 (2H, m), 7.6 (1H, d), 7.65 (1H, d).
후처리
- temperatureAfter 90 min the mixture was cooled
- extractionextracted with hexane (40 ml)
- dry with materialThe hexane layer was dried (MgSO4)
- customevaporated to dryness
- customThe residue was purified by column chromatography on silica gel eluting with 0-30% dichloromethane in hexane
출처 및 근거
- ORD 기록
- ord-bdaed1af101f4a3fb37531108d241fdc
- 출처 데이터셋
- uspto-grants-2001_11
- 특허 번호
- US06320051B1
연결된 노트
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